ANALYTICAL LETTERS
·
2025
·
IF 1.8
Yating Liu,Li Tian,Yuan Gao,Zhonghai Tang,Yuzhu Xiong
An attapulgite-multi-walled carbon nanotube (ATP-CNTs) composite material was synthesized to enhance the QuEChERS method. When coupled with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), an accurate, rapid, and reliable analytical method was established for the determination of multiple pesticide residues in tea. The ATP-CNTs purification agent was characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM). Pesticides in tea were extracted under ultrasonication using water and acetonitrile, followed by purification with ATP-CNTs. Key experimental parameters—including extraction solvent, extraction time, soaking time, soaking water temperature, adsorbent combination ratio, and adsorbent amount—were systematically optimized. Under optimal conditions, the method’s limits of detection (LOD) and quantification (LOQ) were 1.05–4.11 μg/kg and 3.49–13.69 μg/kg, respectively. Recovery experiments at three spiked concentration levels yielded average recoveries ranging from 75.2% to 114.3%, with relative standard deviations (RSDs) between 2.3% and 13.8%. The results demonstrate that this method is simple, accurate, rapid, and suitable for the detection of relevant pesticide residues in tea.
研究领域:
分析化学
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环境科学
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食品科学
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纳米技术
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DOI
高影响因子
Natural Product Communications
·
2020
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IF 0.468
Na Li,Ting Lv,Jie Pan,Chunhua Liu,Jia Sun,Yanyu Lan,Aimin Wang,Yongjun Li,Yonglin Wang,Yuan Lu
A simple, rapid, and selective ultra-performance liquid chromatography-mass spectrometry (MS)/MS method was established to investigate tissue distribution of 6 polyphenolic compounds of Polygonum orientale L. extract in normal and myocardial ischemia (MI) model rat tissues, including isoorientin, orientin, vitexin, quercitrin, astragalin, and protocatechuic acid. An Agilent Eclipse Plus C18 column was used. The mobile phase consisted of acetonitrile and water, both with 0.1% formic acid. Quantification was performed in negative ion multiple reaction monitoring mode. All the analysts had good linearity with r ≥ 0.9912. Accuracy ranged from 12.49% to −13.98% for the 6 compounds; within-day variation (precision) was ≤9.98% and interday precision was ≤11.88%. Extraction recovery of the analysts ranged from 80.55% to 99.92%; the matrix was 81.00%–98.73%. The analyst preparations were stable throughout. The 6 compounds were rapidly distributed in various tissues after oral administration, without accumulation over 12 hours. Compared with normal rats, distributions of 6 compounds in the heart, liver, spleen, lung, kidney, brain, stomach, and intestine in MI model rats were different from those in the normal group. The study provides an insight for further research of P. orientale L.
研究领域:
药理学
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分析化学
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心脏病学
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DOI
高影响因子
MOLECULES
·
2022
·Vol. 27
·期 20
·6952
·
IF 4.927
Liqiong Sun,Zhijuan Tang,Minxin Wang,Jun Shi,Yajuan Lin,Tiefeng Sun,Zhilu Zou,Zebin Weng
With the abuse of antibiotics, bacterial antibiotic resistance is becoming a major public healthcare issue. Natural plants, especially traditional Chinese herbal medicines, which have antibacterial activity, are important sources for discovering potential bacteriostatic agents. This study aimed to develop a fast and reliable method for screening out antimicrobial compounds targeting the MRSA membrane fromPsoralea corylifoliaLinn. seed. A UPLC-MS/MS method was applied to identify the prenylated flavonoids in major fractions from the extracts ofPsoralea corylifoliaLinn. seed. The broth microdilution method was used to determine the minimum inhibitory concentrations (MICs) of different fractions and compounds. The morphological and ultrastructural changes of MRSA were determined by scanning electron microscopy (SEM). The membrane-targeting mechanism of the active ingredients was explored by membrane integrity assays, membrane fluidity assays, membrane potential assays, ATP, and ROS determination. We identified eight prenylated flavonoids inPsoralea corylifoliaLinn. seed. The antibacterial activity and mechanism studies showed that this type of compound has a unique destructive effect on MRSA cell membranes and does not result in drug resistance. The results revealed that prenylated flavonoids inPsoralea corylifoliaLinn. seeds are promising candidates for the development of novel antibiotic agents to combat MRSA-associated infections.Keywords:methicillin-resistantStaphylococcus aureus;Psoralea corylifoliaLinn. seed;prenylated flavonoids;UPLC-MS/MS;bacterial membrane
研究领域:
微生物学
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药理学
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中药学
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DOI
PubMed
高影响因子
BIOCHEMICAL SYSTEMATICS AND ECOLOGY
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2026
·
IF 2.2
Tianze Xin,Yuqing Xu,Bixian Han,Zuoqing Li,Quansheng Liu,Hanxiang Li,Bingqiang Xu
Pleuropterus multiflorus and P. angulatus are two morphologically similar taxa widely used in traditional Chinese medicine but often confused in the herbal market. Their taxonomic relationship remains controversial, and chemical profiling provides complementary evidence for clarifying species boundaries. In this study, an untargeted UPLC–MS/MS approach combined with molecular networking (MN) and multivariate statistical analysis was employed to compare the leaf metabolomes of P . multiflorus and P. angulatus . A total of 46 flavonoid metabolites were structurally annotated, and 16 differential metabolites were identified as key contributors to their separation. MN analysis revealed that both taxa shared the same flavonol core structures, but differed markedly in modification diversity. P. angulatus exhibited a higher abundance of acylated flavonol glycosides and several biflavonoid dimers, whereas P . multiflorus was dominated by non-acylated glycosides. Eight previously unreported structural analogues were also annotated through MN-guided analysis. These compositional and structural differences, observed under common garden conditions, suggest a genetic basis for the metabolic variation. Although limited to the studied accessions, these findings provide preliminary chemophenetic evidence supporting the differentiation of P. angulatus from P. multiflorus . The integration of UPLC–MS/MS and MN demonstrates strong potential for resolving chemical variation among closely related taxa and contributes to improved species authentication, quality control, and conservation of medicinal plant resources.
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高影响因子
Analytical Methods
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2025
·
IF 2.6
Ling Sui,Qiuying Dong,Yudie Lu,Jinqiang Yan,Shuo Zhang,Jinmei Shi,Lixin Yang,Hongmei Shi
During the metabolic process of benzene and its derivatives in living organisms, a series of metabolic products are produced. These metabolites have significant application value in environmental monitoring, occupational health and disease diagnosis. The detection of specific metabolites of benzene series substances can accurately reflect the true level of exposure. In this study, a method based on UPLC-MS/MS was developed for the determination of eight benzene biometabolites in urine. The target substances in urine samples were extracted using HLB columns, separated by gradient elution with HSS T3 liquid chromatography columns, and detected by tandem mass spectrometry. The results showed good linearity in the linear range with correlation coefficients greater than 0.999 for all eight substances.The recoveries were all in the range of 80%~120%, and the detection limits were lower than 0.011 ng/ml.The method is simple to operate, the accuracy and precision meet the detection requirements, and can be applied to the detection of real samples.
研究领域:
环境监测
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职业健康
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毒理学
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分析化学
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DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2022
·Vol. 37
·期 1
·e5525
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IF 1.911
Yuhao Fu,Ying Li,Yinling Ma,Xueru He,Xuejiao Xun,Yanjun Cui,Liju Fan,Zhanjun Dong
Almonertinib was included in the first-line treatment of non-small cell lung cancer with EGFR T790M mutations by the Chinese Society of Clinical Oncology in 2021. Considering that immunocompromised lung cancer patients are prone to opportunistic fungal infections, and most triazole antifungal drugs are moderate or strong inhibitors of CYP3A4, this study was conducted to develop and validate an accurate and rapid ultra-performance liquid chromatography tandem mass spectrometry method for quantifying almonertinib in plasma and for investigating the pharmacokinetic changes of almonertinib caused by voriconazole and fluconazole in rats. After liquid–liquid extraction with tert -butyl methyl ether, an XSelect HSS T3 column (2.1 × 100 mm, 2.5 μm, Waters) was used for the chromatographic separation of almonertinib and sorafenib-D 3 (internal standard). The analytes were detected using an AB Sciex Triple Quad 5,500 mass spectrometer in the positive ionization mode. The method exhibited great linearity (0.5–200 ng/ml, r > 0.997) and stability under the established experimental conditions. All validation experiments were in accordance with the guidelines, and the results were all within the acceptable limits. This method was successfully applied to the researches of pharmacokinetics and drug interactions for almonertinib in rats. Voriconazole and fluconazole significantly altered the pharmacokinetic profiles of almonertinib and increased the systemic exposure of almonertinib in rats to different degrees, but further human trials should be conducted to validate the results.
研究领域:
药理学
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肿瘤学
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分析化学
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DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
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2022
·Vol. 36
·期 4
·e5313
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IF 1.911
Fu-Qin He,Yan-Jun Li,Zhao-Hui Guo,Juan Chen
Cyclocarya paliurus is an edible and medicinal plant exhibiting significant hypoglycemic effect. However, its active components are still unclear and need further elucidation. In this research, the active components of the leaves of C. paliurus responsible for the α -glucosidase inhibitory activity were screened and identified based on a spectrum–effect relationship study in combination with ultra-performance liquid chromatography tandem mass spectrometry (UPLC–MS/MS) analysis. The 70% ethanol eluate fraction of the leaves of C. paliurus with the strongest α -glucosidase inhibitory activity was obtained after extraction and purification with macroporous resin. Their chromatographic fingerprints (15 batches) were established by UPLC analysis and 32 common peaks were specified by similarity analysis. Their IC 50 values for α -glucosidase inhibition were measured by an enzymatic reaction. Several multivariate statistical analysis methods including hierarchical cluster analysis, principal component analysis, partial least square analysis and gray relational analysis were applied to explore the spectrum–effect relationship between common peaks and IC 50 values, and the chromatographic peaks making a large contribution to efficacy were screened out. To further elucidate the active components of leaves of C. paliurus , the 70% ethanol eluate fraction was characterized by UPLC–MS/MS analysis, and 10 compounds were identified. This study provides a valuable reference for further research and development of hypoglycemic active components of C. paliurus .
研究领域:
药理学
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分析化学
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植物科学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2023
·
IF 4.1
Congyang Ding,Caihui Guo,Lingzhi Fang,Yajing Li,Zhi Wang,Zhanjun Dong
Vericiguat (VER) is a novel soluble guanylate cyclase stimulator treating symptomatic chronic heart failure (HF), and it is a substrate of both transporters P-glycoprotein and breast cancer resistance protein (BCRP). Astragaloside IV (ASIV) is the main active ingredient in Radix Astragali (Huangqi), a traditional Chinese medicine widely used for HF treatment in China. ASIV's effect on the protein expression of P-glycoprotein and BCRP has been observed, its impact on VER metabolism remain uncertain. In the present study, male Sprague-Dawley rats were administered with 20 mg/kg ASIV and 1 mg/kg VER to study their pharmacokinetics. Blood samples were subject to liquid-liquid extraction, and riociguat was employed as the internal standard (IS). The analytical method involved a C18 column (XSelect® HSS T3 column, 2.1 × 100 mm, 2.5 μm) with a mobile phase of 0.1% formic acid and acetonitrile for gradient elution. The flow rate of the mobile phase was set at 0.2 mL/min, and 5 µL of the sample was used for analysis. The positive ion multi-response monitoring mode was utilized with a transition of m/z 427.4→109.1 for VER and m/z 423.3→109.1 for the IS. The method exhibited good linearity within the concentration range of 0.1 to 300 ng/mL ( r = 0.9987), and all the validation processes were conducted in accordance with the requirements of biological analysis. The pharmacokinetic results revealed that ASIV did not significantly alter the main parameters of VER, except for C max , which decreased by 33.2% (P < 0.05). Overall, our study successfully established a selective, sensitive and repeatable ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) analysis for detecting VER in rat plasma.
研究领域:
药理学
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分析化学
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中药学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2024
·
IF 3.1
Hualu Wu,Saili Xie,Xiaohai Chen,Hailun Xia,Yuxin Shen,Ren-ai Xu,Wei Tan,Ruanjuan Zhan
Fuzuloparib is a novel orally bioactive poly-ADP-ribose polymerase inhibitor (PARPi), which was approved by the Chinese Regulatory Agency (CRA) in 2020 for the treatment of platinum-sensitive recurrent ovarian, fallopian tube, and primary peritoneal cancers. This study firstly presents a rapid and accurate ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method for analyzing the levels of fuzuloparib and its major metabolite (SHR165202), and to investigate drug-drug interaction between fuzuloparib and curcumin in vitro and in vivo studies. After protein precipitation with acetonitrile, mobile phase consisted of acetonitrile and 0.1 % formic acid with a gradient elution was used to successfully separate fuzuloparib, SHR165202 and talazoparib (internal standard, IS). The results indicated that fuzuloparib and SHR165202 had good linearity over the calibration range of 2–50 ng/mL and 1–20 ng/mL, respectively. The precision, accuracy, stability, matrix effect, and extraction recovery required for methodological validation all complied with the requirements of the Bioanalytical Method Validation Guidelines. In vitro microsome incubation experiments, curcumin exhibited inhibitory effect on fuzuloparib in both rat liver microsomes (RLM) and human liver microsomes (HLM) with half-maximal inhibitory concentration (IC 50 ) value of 10.54 μM and 47.64 μM, respectively, and the corresponding mechanism was non-competitive. Furthermore, the inhibitory mechanism of curcumin on fuzuloparib was validated through molecular docking. In pharmacokinetic experiments in rats, curcumin significantly altered the plasma exposure of fuzuloparib, resulting in significant increases in AUC (0-t) and C max of fuzuloparib and a significant decrease in CL z/F . Moreover, the metabolite SHR165202 showed significant increases in AUC (0-t) , AUC (0-∞) , T max and C max and a significant decrease in CL z/F . This further supports the notion that curcumin could inhibit the metabolism of fuzuloparib. Therefore, when co-administering fuzuloparib and curcumin in clinic, it is recommended to monitor plasma levels of fuzuloparib and pay close attention to adverse effects. If necessary, the dose of fuzuloparib needs to be reduced.
研究领域:
药理学
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分析化学
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肿瘤学
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产品关联
DOI
PubMed
高影响因子
MOLECULES
·
2025
·Vol. 30
·期 4
·852
·
IF 4.6
Qiqi Jin,Qianwen Xu,Zhiyong Zhao,Wenshuai Si,Bing Bai,Lei Chen,Changyan Zhou
This study presents a method for the simultaneous determination of six acidic herbicides and their metabolites in various matrices, including fruits, vegetables, grains, and edible oils. The method employs acidified acetonitrile extraction combined with dispersive solid-phase extraction cleanup (dSPE) using MgSO4, Florisil, and Graphitized carbon black (GCB). The analysis was performed by ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS) with electrospray ionization (ESI) in both positive and negative modes using multiple reaction monitoring (MRM). The mass concentrations of six herbicide pesticides and their metabolites were predominantly within the range of 0.0005~0.050 mg/L and exhibited strong linear relationships with the corresponding peak area, with the coefficient of determination (R2) exceeding 0.993. The limits of detection (LOD) for the method ranged from 0.0001 to 0.008 mg/kg. The recovery rates of adding recovery experiments to cabbage, chives, pear, wheat flour, and soybean oil were 69.8~120%, and the relative standard deviation (RSD) was 0.6~19.5%. The results indicate that this method is efficient and fast, and can be used for the detection of compounds in various actual matrices.
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PubMed
高影响因子
Journal of Pharmaceutical Analysis
·
2017
·
IF 0
Jing Zeng,Hua lin Cai,Zhi ping Jiang,Qing Wang,Yan Zhu,Ping Xu,Xie lan Zhao
A sensitive, rapid, simple and economical ultra-performance liquid chromatography–tandem mass spectrometric method (UPLC–MS/MS) was developed and validated for simultaneous determination of imatinib, dasatinib and nilotinib in human plasma using gliquidone as internal standard (IS). Liquid-liquid extraction method with ethyl acetate was used for sample pre-treatment. The separation was performed on an Xtimate Phenyl column using isocratic mobile phase consisting of A (aqueous phase: 0.15% formic acid and 0.05% ammonium acetate) and B (organic phase: acetonitrile) (A:B=40:60, v/v). The flow rate was 0.25 mL/min and the total run time was 6 min. The multiple reaction monitoring (MRM) transitions, m/z 494.5→394.5 for imatinib, 488.7→401.5 for dasatinib, 530.7→289.5 for nilotinib and 528.5→403.4 for IS, were chosen to achieve high selectivity in the simultaneous analyses. The method exhibited great improvement in sensitivity and good linearity over the concentration range of 2.6–5250.0 ng/mL for imatinib, 2.0–490.0 ng/mL for dasatinib, and 2.4–4700.0 ng/mL for nilotinib. The method showed acceptable results on sensitivity, specificity, recovery, precision, accuracy and stability tests. This UPLC–MS/MS assay was successfully used for human plasma samples analysis and no significant differences were found in imatinib steady-state trough concentrations among the SLC22A5 −1889T>C or SLCO1B3 699G>A genotypes ( P >0.05). This validated method can provide support for clinical therapeutic drug monitoring and pharmacokinetic investigations of these three tyrosine kinase inhibitors (TKIs).
研究领域:
药理学
·
临床医学
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分析化学
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DOI
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
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2015
·
IF 2.729
Min Liao,Xiao Chen,Jiefeng Chen,Mengping Liu,Junyi Wang,Zuanguang Chen,Zhiyong Xie,Meicun Yao
An original and sensitive ultraperformance liquid chromatography–tandem mass spectrometric (UPLC–MS/MS) method for the determination of pseudoprotodioscin (PPD) in rat plasma was developed and validated. Digitoxin was applied as an internal standard. Plasma samples were processed by acetonitrile-mediated plasma protein precipitation and chromatographed using a step gradient program on a C18 column (2.1 × 50 mm i.d., 1.7 μm). The mobile phase was comprised of acetonitrile and 0.1 mmol L −1 aqueous lithium acetate mixed with 0.03% formic acid at the flow rate of 0.2 mL min −1 . Multiple reaction monitoring (MRM) transitions were performed for detection and lithium adduct ions were employed with a significant improvement of the response of the analytes in electrospray positive ionization mode. The concentration range of calibration curve was linear over the range 2–5000 ng mL −1 . The intra- and inter-day precisions were all less than 11.5% and accuracies were within the range of 94.1–103.5%, and the analytes exhibited no severe matrix effect. The validated method was successfully applied in the pharmacokinetics of PPD after intragastric (50 mg kg −1 ) and intravenous (4 mg kg −1 ) administration in rats. PPD showed rapid excretion and with bioavailability of simply about 5.7% in rats.
研究领域:
分析化学
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药理学
·
中药学
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产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）